论文部分内容阅读
目的:建立液质联用(LC-MS)法测定人体血浆特拉唑嗪的浓度及应用。方法:岛津LC-MS2010液相色谱-质谱联用仪,色谱柱为Thermo Hypersil-Hypurity C18(150mm×2.1mm,5μm);柱温:40℃;流动相为20mmmol/L乙酸铵溶液(pH4.3)∶甲醇∶乙腈=65∶20∶15;流速:0.25mL/min。采用电喷雾正离子模式离子化,用于定量分析的离子分别为m/z388(特拉唑嗪)、m/z384(哌唑嗪)。血浆样品采用3mol/L氢氧化钠碱化、二氯甲烷萃取后LC-MS测定。进样体积为5μL,样品室温度为5℃。结果:特拉唑嗪线性范围为0.25～50ng/mL,最小定量浓度为0.25ng/mL,提取回收率均>70%,方法回收率为96.0%～97.6%,日间、日内RSD均<15%。方法灵敏、稳定、特异性高,并已成功地应用到人体血浆特拉唑嗪药代动力学的研究。结论:该方法简便、准确、重复性好,可以准确地定量人体血浆特拉唑嗪的浓度,适于特拉唑嗪生物利用度和生物等效性的研究。
Objective: To establish a liquid chromatography-mass spectrometry (LC-MS) method for the determination of plasma concentration and its application of terazosin in human plasma. Methods: Shimadzu LC-MS2010 liquid chromatography-mass spectrometer, the column was Thermo Hypersil-Hypquis C18 (150mm × 2.1mm, 5μm); the column temperature was 40 ℃; the mobile phase was 20mmmol / L ammonium acetate solution .3): methanol: acetonitrile = 65: 20: 15; flow rate: 0.25 mL / min. The ions were ionized by electrospray positive ion mode and used for quantitative analysis. The ions were m / z 388 (terazosin) and m / z 384 (prazosin) respectively. Plasma samples were alkalinized with 3 mol / L sodium hydroxide and analyzed by LC-MS after dichloromethane extraction. The injection volume was 5 μL and the sample compartment temperature was 5 ° C. Results: The linear range of terazosin was 0.25 ~ 50ng / mL, the minimum concentration was 0.25ng / mL. The recoveries were both> 70%. The recoveries were between 96.0% and 97.6% %. The method is sensitive, stable and specific and has been successfully applied to the study of pharmacokinetics of terazosin in human plasma. Conclusion: The method is simple, accurate and reproducible. It can accurately measure the plasma concentration of terazosin in human plasma and is suitable for the study of bioavailability and bioequivalence of terazosin.